CN114436315A - Preparation method of nano dysprosium oxide and nano dysprosium oxide prepared by same - Google Patents

Preparation method of nano dysprosium oxide and nano dysprosium oxide prepared by same Download PDF

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CN114436315A
CN114436315A CN202011231660.2A CN202011231660A CN114436315A CN 114436315 A CN114436315 A CN 114436315A CN 202011231660 A CN202011231660 A CN 202011231660A CN 114436315 A CN114436315 A CN 114436315A
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dysprosium oxide
dysprosium
nano
water
temperature
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韦家谋
罗冷
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Hunan University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C01F17/224Oxides or hydroxides of lanthanides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/10Preparation or treatment, e.g. separation or purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention provides a preparation method of nano dysprosium oxide, which comprises the following steps: s1, preparing slurry; s2, adding water into the slurry, performing ball milling, and screening by a filter screen of 80 meshes to obtain uniform emulsion/suspension; s3, dripping the emulsion/suspension obtained in the step S2 into a drying device under the stirring state for spray drying, and obtaining dry powder with the water content not higher than 20 wt%; and S4, calcining the dried powder obtained in the step S3 in a furnace body, and cooling to room temperature after calcination to obtain the nano dysprosium oxide. The invention takes insoluble dysprosium salt as a raw material, and can obtain the nano dysprosium oxide with small particle size and uniform particle size distribution. The invention also provides a nano dysprosium oxide.

Description

Preparation method of nano dysprosium oxide and nano dysprosium oxide prepared by preparation method
Technical Field
The invention relates to the field of material preparation, and particularly provides a preparation method of nano dysprosium oxide. The invention also provides a nano dysprosium oxide.
Technical Field
Dysprosium oxide is an additive for preparing raw materials of metal dysprosium, glass and neodymium iron boron permanent magnets, and is also used in metal halogen lamps, magneto-optical memory materials, yttrium iron or yttrium aluminum garnet and atomic energy industries and used as a control rod of nuclear power reactors. With the development of science and technology, the demand of the large specific surface area nano dysprosium oxide is more and more, and in a ceramic electric melter, the nano dysprosium oxide particles can obviously improve the performance of products.
The patent application of the comparison document 1CN105502467A discloses a preparation method of nano dysprosium oxide, and specifically discloses that dysprosium nitrate with the concentration of 0.1-0.6 mol/L prepared by pure water is added into a reaction kettle, then analytically pure sodium carbonate with the concentration of 0.1-0.6 mol/L prepared by pure water is weighed, and the mass ratio of the dysprosium nitrate to the analytically pure sodium carbonate is 1:1-1: 1.2; weighing 5-15% by mass of polyethylene glycol 2000 surfactant, adding the surfactant into dysprosium nitrate, stirring for 15-30min, uniformly dropwise adding a precipitator, stirring, aging, carrying out suction filtration, washing with water, filtering, drying, adding surfactant n-butyl alcohol, and uniformly stirring, wherein the mass ratio of the obtained substance to the n-butyl alcohol is 1:200-1: 400; then burning at 800 ℃ for 3-5h and keeping the temperature for 1h to obtain the nano dysprosium oxide with the particle size of 40-60nm and the specific surface area of more than 25. Dysprosium oxide with the particle size of 40-60nm is prepared by the application of the patent, dysprosium nitrate and sodium carbonate are used as raw materials in the method, a precipitator is added to prepare a precursor, a large amount of n-butyl alcohol serving as a surfactant is used in the process, the production cost is increased, the method is not environment-friendly, and the size of dysprosium oxide crystal grains cannot be controlled. The patent of the comparison document 2CN105314667B discloses a method for preparing ultrafine uniform dysprosium oxide, which specifically discloses weighing dysprosium oxide powder, putting the dysprosium oxide powder into a reaction kettle, adding pure water, mixing and stirring uniformly, adding a nonionic surfactant, and stirring at a constant speed to obtain a completely infiltrated mixture; adding zirconium beads into a high-energy grinding machine, adding the soaked mixture into the grinding machine, and grinding to obtain slurry with uniform dispersibility; the uniformly dispersed slurry is contained in a charging basket container, one end of a peristaltic pump is connected with the charging basket container, the other end of the peristaltic pump is connected with a dryer, the slurry is sprayed into the dryer in a mist shape through the peristaltic pump, the sprayed slurry is dried in the dryer, and a dried product collected from the dryer is ultrafine-particle dysprosium oxide. In the patent, dysprosium oxide and a surfactant are directly mixed and ball-milled, and spray-dried to obtain dysprosium oxide of 0.2-0.45um, wherein the dysprosium oxide is easy to form agglomeration because of not being subjected to high-temperature treatment in the manufacturing process, and the size of dysprosium oxide crystal grains cannot be controlled.
In summary, the dysprosium oxide particle size precipitated by oxalic acid by utilizing the traditional method in the rare earth industry is generally in the range of 1-15 μm, while ammonia water, ammonium carbonate and the like are precipitated, so that the preparation cannot be carried out due to adverse environmental protection, the concentration of a reaction system is not uniform due to other preparation methods of the dysprosium oxide nano-particles, the growth speed of dysprosium ions is difficult to control, and the prepared dysprosium oxide powder has wide particle size distribution range and large particle size; in addition, the preparation method has complicated steps and complicated equipment, various variables need to be controlled, the particle size distribution range of the powder is not adjustable, and the nano dysprosium oxide prepared by the hydrothermal method has serious agglomeration phenomenon and difficult separation.
Disclosure of Invention
In order to solve the problems that the particle size distribution range of the product in the prior art is not adjustable, the environmental pollution is easily caused and the steps are complicated, the invention provides a preparation method of nano dysprosium oxide and the nano dysprosium oxide prepared by the preparation method, and provides a method for preparing nano dysprosium oxide powder by taking insoluble dysprosium salt as a raw material, adding fluxing salt and adopting a simple high-temperature calcination process means.
A preparation method of nano dysprosium oxide comprises the following steps:
s1, adding the molten salt into water, stirring until the molten salt is dissolved, adding the dispersing agent and the surfactant, and mixing to obtain a mixed solution; gradually adding the mixed solution into a certain amount of dysprosium salt insoluble in water, and mechanically stirring until the mixed solution is uniformly dispersed to obtain required slurry; wherein the mass ratio of the dysprosium salt to the molten salt is 1: 0.01-5; the mass ratio of the dysprosium salt to the water is 1: 0.1-5;
s2, adding water into the slurry, performing ball milling, and screening by a filter screen of 80 meshes to obtain uniform emulsion/suspension; wherein the mass ratio of the slurry to the water is 0.5-4: 1;
s3, dripping the emulsion/suspension obtained in the step S2 into a drying device under the stirring state for spray drying, and obtaining dry powder with the water content not higher than 20 wt%;
s4, calcining the dried powder obtained in the step S3 in a furnace body, wherein the calcining stage comprises the following steps: the temperature is kept at the highest temperature for 0-300 min from room temperature to 400 ℃, with the heating rate of 0.1-50 ℃/min, 400-600 ℃, 0.1-50 ℃/min, 600-900 ℃, 0.1-50 ℃/min; cooling to room temperature after calcining to obtain the nano dysprosium oxide.
Further, the dispersant in step S1 is polyethylene glycol.
Further, the surfactant in step S1 is one or more of cetyltrimethylammonium bromide, polyethylene glycol, stearic acid and quaternary ammonium compound.
Further, the dysprosium salt insoluble in water in step S1 is dysprosium carbonate, dysprosium acetate and dysprosium oxalate.
Further, in step S1, the molten salt is one or more of ammonium chloride, sodium chloride, potassium chloride, sodium fluoride, ammonium carbonate, ammonia water, sodium carbonate, potassium carbonate, ammonium citrate, sodium citrate, or potassium citrate.
Further, in step S2, the ball milling time is 5 to 10min, preferably 8 min.
Further, in step S3, the temperature of spray drying is 100 to 200 ℃, preferably 115 ℃.
The invention also provides nano dysprosium oxide prepared by the preparation method of the nano dysprosium oxide.
Has the advantages that:
1. the invention adopts the dysprosium carbonate, the dysprosium acetate, the dysprosium oxalate and other insoluble salts as main raw materials and adopts a special calcination technology, thereby obtaining dysprosium oxide particles with the minimum size of 50 nanometers, uniform particle size, good dispersibility, high calcination temperature and complete crystal growth.
2. The preparation method of the nano dysprosium oxide is simple and stable, has few working procedures, has low requirements on equipment, uses few raw materials, generates tail gas which is easy to absorb and treat, has no toxicity or pollution, and has low production cost; in addition, the produced nano dysprosium oxide is in a sphere-like shape, has high purity, is not agglomerated, has narrow particle size distribution and is easy to disperse by adding polyethylene glycol and a certain amount of surfactant.
3. The nano dysprosium oxide obtained by the invention can be applied to the aspects of high-grade ceramics, neodymium iron boron permanent magnets and the like.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the scope of protection of the present invention.
Example 1
The invention provides a preparation method of nano dysprosium oxide, which comprises the following steps:
s1, adding the molten salt into water, stirring until the molten salt is dissolved, adding the dispersing agent and the surfactant, and mixing to obtain a mixed solution; gradually adding the mixed solution into a certain amount of dysprosium salt insoluble in water, and mechanically stirring until the mixed solution is uniformly dispersed to obtain required slurry; wherein the mass ratio of the dysprosium salt to the molten salt is 1: 0.01-5; the mass ratio of the dysprosium salt to the water is 1: 0.1-5;
s2, adding water into the slurry, performing ball milling, and screening by a filter screen of 80 meshes to obtain uniform emulsion/suspension; wherein the mass ratio of the slurry to the water is 0.5-4: 1;
s3, dripping the emulsion/suspension obtained in the step S2 into a drying device under the stirring state for spray drying, and obtaining dry powder with the water content not higher than 20 wt%;
s4, calcining the dried powder obtained in the step S3 in a furnace body, wherein the calcining stage comprises the following steps: the temperature is kept at the highest temperature for 0-300 min from room temperature to 400 ℃, with the heating rate of 0.1-50 ℃/min, 400-600 ℃, 0.1-50 ℃/min, 600-900 ℃, 0.1-50 ℃/min; cooling to room temperature after calcining to obtain the nano dysprosium oxide.
In this embodiment, the mass of the dispersant and the surfactant is one thousandth to ten thousandth of the mass of the solid raw material, respectively, and in a preferred embodiment, the mass of the dispersant and the surfactant is three thousandth of the fixed mass of the raw material, respectively.
In this embodiment, the mechanical stirring and dispersing manner used in step S1 is mechanical stirring at room temperature, and the mechanical stirring and dispersing function is to sufficiently mix and disperse the molten salt with the dysprosium salt insoluble in water uniformly so that the molten salt is adsorbed on the surface of the dysprosium salt insoluble in water;
in the step S2, the ball milling time is 5-10 min, preferably 8 min; the ball milling has the following functions: so that the molten salt is more uniformly and comprehensively adsorbed on the surface of the dysprosium salt which is insoluble in water; because the dysprosium salt insoluble in water is dissociated under the action of mechanical force, free electrovalence bonds can be generated on the new section, and particle molecules are aggregated with each other, so that the dysprosium oxide obtained after calcination is more seriously aggregated, and positive and negative ions generated by dissociation of a molten salt solution in an aqueous solution can be adsorbed on the surface of a ball-milled product, thereby preventing the aggregation phenomenon of the particles;
the spray drying temperature in the step S3 is 100-200 ℃, and preferably 115 ℃; the spray drying is adopted to aim at refining and homogenizing the precursor, so that the molten salt can be conveniently and uniformly and effectively adsorbed on the surface of dysprosium salt which is insoluble in water;
in step S4, the crystallization of the nano dysprosium oxide is promoted and the size of the crystal grains of the nano dysprosium oxide can be controlled by the calcination temperature, the time for raising the temperature to the maximum temperature and the time for holding the maximum temperature, wherein the holding time for the maximum temperature is 30-90 min, and the calcination process specifically comprises the following steps: from room temperature to 400 ℃, the heating rate is 0.1-50 ℃/min, the heating time is 0-90 min, the preheating process activates the raw materials, particularly molten salt, and part of the molten salt begins to dissolve or decompose; the temperature is 400-600 ℃, the heating rate is 0.1-50 ℃/min, the heating time is 0-90 min, and the molten salt accelerates the decomposition kinetic rate of dysprosium salt insoluble in water and promotes the crystallization of dysprosium oxide; the molten salt is decomposed at high temperature, and the generated ascending hot air flow can break partial agglomeration or dysprosium salt or dysprosium oxide with agglomeration tendency to a certain extent; the growth and agglomeration of dysprosium oxide crystal nuclei are effectively prevented, and the molten salt also retains the dispersion function of dysprosium oxide particles by a grinding aid mechanism; 600-900 ℃, the heating rate is 0.1-50 ℃/min, the heating time is 0-90 min, the time period aims at the rapid forming of dysprosium oxide crystal nuclei and the growth of crystal grains, the high temperature enables the rapid forming of the dysprosium oxide crystal nuclei, the existence of molten salt effectively prevents the growth and agglomeration of the dysprosium oxide crystal nuclei, and the particle size of particles is controlled to a certain extent; promoting the crystallization of dysprosium oxide and controlling the size of dysprosium oxide crystal grains by constant temperature and time; finally, the temperature is reduced along with the furnace body or is quickly reduced to prepare the nano dysprosium oxide; the furnace body used for calcining is a muffle furnace, a tubular furnace, a rotary furnace, a crucible resistance furnace, a box furnace, a lifting furnace, a well furnace, a trolley furnace, a mesh belt furnace, a roller kiln, a push plate kiln, a tunnel furnace, a rotary kiln, a suspension calcining furnace or the calcining equipment with atmosphere.
The invention also provides nano dysprosium oxide prepared by the preparation method of the nano dysprosium oxide.
Example 2
In this embodiment, 1.75g of ammonium chloride is uniformly dissolved in 7.5g of deionized water at 90 ℃, 0.025g of polyethylene glycol and 0.025g of cetyltrimethylammonium bromide are added, one of the materials is slowly poured into 25g of dysprosium carbonate while being stirred to obtain slurry, the slurry and a certain amount of deionized water are put into a ball mill to be ball-milled for 8min at a rotating speed of about 400r/min, the ball-milled slurry is filtered through a filter sieve of 80 meshes and is washed and sieved by a proper amount of deionized water, and the mass fraction of the obtained emulsion/suspension is controlled to be 40%; then, stirring the emulsion/suspension liquid and spray-drying at the same time, controlling the spray-drying temperature to be 115 ℃ and the feeding amount to be 550ml/h to obtain mixture dry powder, wherein the water content of the powder after spray-drying is not higher than 20 wt%; then placing the mixture powder into a ceramic crucible, placing the ceramic crucible into a muffle furnace, and setting the temperature rise range as follows: the room temperature is 800 ℃, and the temperature rise time is 90 min; the temperature is kept at 800 ℃ for 60 min. Cooling to room temperature along with the furnace, wherein the cooling time is 40min, and the nano dysprosium oxide with the particle size of about 50nm and uniform distribution can be obtained.
Example 3
In this embodiment, 1.75g of ammonium chloride is uniformly dissolved in 7.5g of deionized water at 90 ℃, 0.025g of polyethylene glycol and 0.025g of cetyltrimethylammonium bromide are added, one of the materials is slowly poured into 25g of dysprosium carbonate while being stirred to obtain slurry, the slurry and a certain amount of deionized water are put into a ball mill to be ball-milled for 8min at a rotating speed of about 400r/min, the ball-milled slurry is filtered through a filter sieve of 80 meshes and is washed and sieved by a proper amount of deionized water, and the mass fraction of the obtained emulsion/suspension is controlled to be 40%; then, stirring the emulsion/suspension liquid and spray-drying at the same time, controlling the spray-drying temperature to be 115 ℃ and the feeding amount to be 550ml/h to obtain mixture dry powder, wherein the water content of the powder after spray-drying is not higher than 20 wt%; then placing the mixture powder into a ceramic crucible, placing the ceramic crucible into a muffle furnace, and setting the temperature rise range as follows: the room temperature is 800 ℃, and the temperature rise time is 60 min; the temperature of 800 ℃ is kept for 90 min. Cooling to room temperature along with the furnace, wherein the cooling time is 40min, and the nano dysprosium oxide with the particle size of about 50nm and uniform distribution can be obtained.
Example 4
In this embodiment, 1.75g of ammonium chloride is uniformly dissolved in 7.5g of deionized water at 90 ℃, 0.025g of polyethylene glycol and 0.025g of cetyltrimethylammonium bromide are added, one of the materials is slowly poured into 25g of dysprosium carbonate while being stirred to obtain slurry, the slurry and a certain amount of deionized water are put into a ball mill to be ball-milled for 8min at a rotating speed of about 400r/min, the ball-milled slurry is filtered through a filter sieve of 80 meshes and is washed and sieved by a proper amount of deionized water, and the mass fraction of the obtained emulsion/suspension is controlled to be 40%; then, stirring the emulsion/suspension liquid and spray-drying at the same time, controlling the spray-drying temperature to be 115 ℃ and the feeding amount to be 550ml/h to obtain mixture dry powder, wherein the water content of the powder after spray-drying is not higher than 20 wt%; then placing the mixture powder into a ceramic crucible, placing the ceramic crucible into a muffle furnace, and setting the temperature rise range as follows: heating for 30min at 300-800 ℃; the temperature is kept at 800 ℃ for 60 min. Cooling to room temperature along with the furnace for 40min to obtain the nano cerium-zirconium solid solution with the particle size of 100-200 nm and uniform distribution. In the embodiment, during the calcination process, the initial temperature of the calcination is 300 ℃, and the rapid heating is started from 300 ℃, because the rapid heating is favorable for the rapid progress of the reaction, the severity of the reaction is aggravated, and the particles can be rapidly molded to obtain the dysprosium oxide nanoparticles with larger particle size.
Example 5
In this embodiment, 1.75g of sodium chloride is uniformly dissolved in 7.5g of deionized water at 90 ℃, 0.025g of polyethylene glycol and 0.025g of cetyltrimethylammonium bromide are added, one of the materials is slowly poured into 25g of dysprosium carbonate while being stirred to obtain slurry, the slurry and a certain amount of deionized water are put into a ball mill to be ball-milled for 8min at a rotating speed of about 400r/min, the ball-milled slurry is filtered through a filter sieve of 80 meshes and is washed and sieved by a proper amount of deionized water, and the mass fraction of the obtained emulsion/suspension is controlled to be 40%; then, stirring the emulsion/suspension liquid and spray-drying at the same time, controlling the spray-drying temperature to be 115 ℃ and the feeding amount to be 550ml/h to obtain mixture dry powder, wherein the water content of the powder after spray-drying is not higher than 20 wt%; then placing the mixture powder into a ceramic crucible, placing the ceramic crucible into a muffle furnace, and setting the temperature rise range as follows: the room temperature is 800 ℃, and the temperature rise time is 90 min; the temperature is kept at 800 ℃ for 60 min. Cooling to room temperature along with the furnace, wherein the cooling time is 40min, and the nano dysprosium oxide with the particle size of 200-300 nm and uniform distribution can be obtained. In this embodiment, the molten salt is sodium chloride, and the sodium chloride is in an ion-melting state at a high temperature, and interacts with the dysprosium oxide material to obtain the dysprosium oxide nanoparticles with larger particle sizes.
Example 6
In this embodiment, 1.75g of sodium chloride is uniformly dissolved in 7.5g of deionized water at 90 ℃, 0.025g of polyethylene glycol and 0.025g of cetyltrimethylammonium bromide are added, one of the materials is slowly poured into 25g of dysprosium carbonate while being stirred to obtain slurry, the slurry and a certain amount of deionized water are put into a ball mill to be ball-milled for 8min at a rotating speed of about 400r/min, the ball-milled slurry is filtered through a filter sieve of 80 meshes and is washed and sieved by a proper amount of deionized water, and the mass fraction of the obtained emulsion/suspension is controlled to be 40%; then, stirring the emulsion/suspension liquid and spray-drying at the same time, controlling the spray-drying temperature to be 115 ℃ and the feeding amount to be 550ml/h to obtain mixture dry powder, wherein the water content of the powder after spray-drying is not higher than 20 wt%; then placing the mixture powder into a ceramic crucible, placing the ceramic crucible into a muffle furnace, and setting the temperature rise range as follows: the room temperature is 900 ℃, and the temperature rise time is 90 min; the temperature of 900 ℃ is kept for 60 min. Cooling to room temperature along with the furnace, wherein the cooling time is 40min, and then the nano dysprosium oxide with the particle size of 300-400 nm and uniform distribution can be obtained.
By comparing the example 2 with the example 3, the particle size of the nano dysprosium oxide is the same under the condition that the calcination time and the maximum temperature are the same, and the temperature holding time is independent of the maximum temperature.
By comparing the example 2 with the example 4, it can be seen that the grain size of the nano dysprosium oxide is larger and the change is larger when the initial temperature is higher and the temperature rise rate is faster under the condition that the maximum temperature and the holding time at the maximum temperature are the same.
By comparing example 2 with example 5, it can be seen that the particle size of the nano dysprosium oxide obtained by using the sodium chloride molten salt is larger than that of the ammonium chloride molten salt under the condition that the calcination time and the holding time at the maximum temperature are the same.
By comparing the example 2, the example 3 and the example 4, the particle size of the nano dysprosium oxide is 50nm at the minimum when the maximum temperature is 800 ℃ from room temperature to the maximum temperature.
By comparing example 5 with example 6, it can be seen that the higher the annealing temperature is, the larger the particle size of the dysprosium oxide nanoparticles is, that is, the higher the maximum temperature is, the larger the particle size of the dysprosium oxide nanoparticles is, when the calcination time and the holding time at the maximum temperature are the same.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The preparation method of nano dysprosium oxide is characterized by comprising the following steps of:
s1, adding the molten salt into water, stirring until the molten salt is dissolved, adding the dispersing agent and the surfactant, and mixing to obtain a mixed solution; gradually adding the mixed solution into a certain amount of dysprosium salt insoluble in water, and mechanically stirring until the mixed solution is uniformly dispersed to obtain required slurry; wherein the mass ratio of the dysprosium salt to the molten salt is 1: 0.01-5; the mass ratio of the dysprosium salt to the water is 1: 0.1-5;
s2, adding water into the slurry, performing ball milling, and screening by a filter screen of 80 meshes to obtain uniform emulsion/suspension; wherein the mass ratio of the slurry to the water is 0.5-4: 1;
s3, dripping the emulsion/suspension obtained in the step S2 into a drying device under the stirring state for spray drying, and obtaining dry powder with the water content not higher than 20 wt%;
s4, calcining the dried powder obtained in the step S3 in a furnace body, wherein the calcining stage comprises the following steps: the temperature is kept at the highest temperature for 0-300 min from room temperature to 400 ℃, with the heating rate of 0.1-50 ℃/min, 400-600 ℃, 0.1-50 ℃/min, 600-900 ℃, 0.1-50 ℃/min; cooling to room temperature after calcining to obtain the nano dysprosium oxide.
2. The method for preparing nano dysprosium oxide according to claim 1, wherein in step S1, the dispersant is polyethylene glycol.
3. A method for preparing dysprosium oxide nanoparticles as claimed in claim 1, wherein in step S1, the surfactant is one or more of cetyltrimethylammonium bromide, polyethylene glycol, stearic acid and quaternary ammonium compound.
4. The method for preparing nano dysprosium oxide according to claim 1, wherein in step S1, the dysprosium salt insoluble in water is dysprosium carbonate, dysprosium acetate and dysprosium oxalate.
5. A method for preparing nano dysprosium oxide according to claim 1, wherein in step S1, the molten salt is one or more of ammonium chloride, sodium chloride, potassium chloride, sodium fluoride, ammonium carbonate, ammonia water, sodium carbonate, potassium carbonate, ammonium citrate, sodium citrate or potassium citrate.
6. The method for preparing dysprosium oxide nanoparticles as claimed in claim 1, wherein in step S2, the ball milling time is 5-10 min.
7. The method for preparing nano dysprosium oxide according to claim 6, wherein the ball milling time is 8 min.
8. A method for preparing dysprosium oxide nanoparticles as claimed in claim 1, wherein in step S3, the temperature of spray drying is 100-200 ℃.
9. The method for preparing nano dysprosium oxide according to claim 8, wherein the temperature of spray drying is 115 ℃.
10. A nano dysprosium oxide, characterized in that the nano dysprosium oxide is prepared by the method for preparing nano dysprosium oxide as claimed in any one of claims 1 to 9.
CN202011231660.2A 2020-11-06 2020-11-06 Preparation method of nano dysprosium oxide and nano dysprosium oxide prepared by same Pending CN114436315A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115246653A (en) * 2022-07-12 2022-10-28 中南大学 Nanometer dysprosium oxide and preparation method and application thereof
CN117185336A (en) * 2023-11-08 2023-12-08 中稀(江苏)稀土有限公司 Controllable preparation method for superfine dysprosium oxide specific surface area

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115246653A (en) * 2022-07-12 2022-10-28 中南大学 Nanometer dysprosium oxide and preparation method and application thereof
CN115246653B (en) * 2022-07-12 2023-10-17 中南大学 Nanometer dysprosium oxide and preparation method and application thereof
CN117185336A (en) * 2023-11-08 2023-12-08 中稀(江苏)稀土有限公司 Controllable preparation method for superfine dysprosium oxide specific surface area
CN117185336B (en) * 2023-11-08 2024-01-16 中稀(江苏)稀土有限公司 Controllable preparation method for superfine dysprosium oxide specific surface area

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